SCD Beamline

What is Single Crystal Diffraction good for?

The aim of X-ray Single Crystal Diffraction (SCD) is the determination of the atomic coordinates in the unit cell of a single crystal. The ANKA-SCD beamline allows structure determination of large crystallized molecules with lattice parameters from about 2 nm to about 20 nm. The largest class of these are biological macromolecules, in particular proteins. Sample sizes typically are between (0.1 mm)3 and (0.5 mm)3. As the energy of the radiation incident onto the sample is tunable over a wide energy range by means of a monochromator, application of the MAD (Multiple Anomalous Dispersion) method for phase determination is feasible. The high incoming photon flux and low beam divergence - as compared to x-ray tubes - allows data acquisition from weakly diffracting crystals or with higher resolution.

Team SCD
	name	titel	function	e-mail
	Buth, Gernot	Dr.	Beamline Scientist - SCD	gernot buthTcm1∂kit edu

Aufbau SCD Beamline

Available Methods, Obtainable Parameters

Single Crystal Diffraction (SCD):
Yields electron density maps and atomic coordinates within the asymmetric unit of the unit cell of a single crystal.

Single / Multiple Anomalous Dispersion (SAD/MAD):
These are special SCD techniques to determine the scattering phases from the anomalous signals of certain elements, e.g. of heavy atoms in vicinity of absorption edges, and thereby solve the phase problem.

Wide Angle X-Ray Scattering (WAXS):
Allows to derive pair correlation functions. This technique, particularly suited for the investigation of structural properties of polymers, provides information about order within the crystalline regions of a sample and about the fraction of crystalline material.

Energy range	4 keV - 20 keV → Ti to Mo K-edge, I to U L-edge ^[1]
Energy resolution [ΔE/E]	Si (111): 3.5 10^-4 @ 9 keV
Source	1.5 T Bending magnet (E_C= 6 keV)
Optics	Flat Rh coated Si mirror with bending mechanism, double crystal monochromator with bender on the 2^nd crystal
Beam size at sample	approx. 2 mm (hor) x 1 mm (ver), depending on focusing conditions
Flux at sample position	Si(111): 3x10⁺¹⁰ ph/s/0.1%bw in 1 mm² @ 9 keV
Experimental setup / sample stage	2 diffractometers with ω, fixed χ, φ - circles
Experimental setup / sample environment	N₂ cryo cooler (80 K - 400 K, 0.1 K accuracy, Oxford Cryosystems)
Experimental setup / detectors	Ø 340 mm Image Plate (STOE IPDS 2) 62 mm x 62 mm CCD ( < 2 seconds total read time), (60 µm)² resolution, Bruker AXS SMART APEX) Energy resolving SDD for fluorescence scans, 140 eV resolution @ 5.9 keV (Ketek AXAS)
Software / Data treatment / Evaluation	X-AREA, X-RED, X-SHAPE, SMART, SAINT, SADABS, XPREP, SHELXTL, CHOOCH

[1] Intensity drops considerably at both ends of the spectrum, below about 6 keV due to air and window absorption and above about 17 keV due to limitations of the DCM crystal bending radius and the bending magnet spectrum.

Publications
Title	Author	Source	Date	List
All-Round Robustness of the Mn19 Coordination Cluster System: Experimental Validation of a Theoretical Prediction	A.M. Ako, Y. Lan, O. Hampe, E. Cremades, E. Ruiz, C.E. Anson, A.K. Powell	Chem. Commun. 50, 5847-5850	2014	PDF
Influence of a low-temperature capping on the crystalline structure and morphology of InGaN quantum dot structures	B. Krause, B. Miljevic, T. Aschenbrenner, E. Piskorska-Hommel, C. Tessarek, M. Barchuk, G. Buth, R. Donfeu Tchana, S. Figge, J. Gutowski, D. Hänschke, J. Kalden, T. Laurus, S. Lazarev, R. Magalhaes-Paniago, K. Sebald, A. Wolska, D. Hommel, J. Falta, V. Holý, T. Baumbach	J. Alloys Comp. 585, 572-579	2014	PDF
Pharmaceutical hydrates under ambient conditions from high-pressure seeds: a case study of GABA monohydrate	F. P. A. Fabbiani, G. Buth, D. C. Levendis, A. J. Cruz-Cabeza	Chem. Commun. DOI: 10.1039/c3cc48466a	2014	PDF
Investigation of the luminescence, crystallographic and spatial resolution properties of nLSO:Tb scintillating layers used for X-ray imaging applications	A. Cecilia, V. Jary, M. Nikl, E. Mihokova, D. Hänschke, E. Hamann, P.-A. Douissard, A. Rack, T. Martin, B. Krause, T. Baumbach, M. Fiederle	Radiat. Meas. DOI: 10.1016/j.radmeas.2013.12.005	2014	PDF
Thermal conductivity of isotopically controlled silicon nanostructures	H. Bracht, S. Eon, R. Frieling, A. Plech, D. Issenmann, D. Wolf, J. Lundsgaard Hansen, A. Nylandsted Larsen, J.W. Ager III, E. E. Haller	New J. Physics 16, 015021	2014	PDF
Three-dimensional reciprocal space profile of an individual nanocrystallite inside a thin-film solar cell absorber layer	T. Slobodskyy, P. Schroth, A. Minkevich, D. Grigoriev, E. Fohtung, M. Riotte, T. Baumbach, M. Powalla, U. Lemmer, A. Slobodskyy	Journal of Physics D: Applied Physics 46, 475104	2013	PDF
Studies on Defect Reduction in AlGaN Heterostructures by Integrating an In-situ SiN Interlayer	F. Scholz, K. Forghani, M. Klein, O. Klein, U. Kaiser, B. Neuschl, I. Tischer, M. Feneberg, K. Thonke, S. Lazarev, S. Bauer, T. Baumbach	Japanese Journal of Applied Physics 52, 08JJ07-1-4	2013	PDF
[Ge12{FeCp(CO)2}8{FeCp(CO)}2]: A Ge12 Core Resembles the Arrangement of the High-Pressure Modification Germanium (II)	C. Schenk, F. Henke, A. Schnepf	Angew. Chem. Int. Ed. 52, 1834-1838	2013	PDF
Crystal structure and packing energy calculations of (+)-6-aminopenicillanic acid	S. Saouane, G. Buth, F. P. A. Fabbiani	Acta Crystallographica Section C 69, 1238-1242	2013	PDF
Evidence of slow relaxation of magnetization in dysprosium-based ionic liquids	D. Prodius, F. Macaev, Y. Lan, G. Novitchi, S. Pogrebnoi, E. Stingaci, V. Mereacre, C. E. Anson, A. K. Powell	Chem. Commun. 49, 9215-9217	2013	PDF
Electrochemical insertion of Li into nanocrystalline MnFe2O4: a study of the reaction mechanism	S. Permien, H. Hain, M. Scheuermann, S. Mangold, V. Mereacre, A. K. Powell, S. Indris, U. Schürmann, L. Kienle, V. Duppel, S. Harma, W. Bensch	RSC Adv. 3, 23001-23014	2013	PDF
Application of GaCp as a Ligand in Coordination Chemistry: Similarities and Differences to GaCp	D. Naglav, B. Tobey, A. Schnepf	Eur. J. Inorg. Chem. 2013, 4146-4149	2013	PDF
A contribution to the crystal chemistry of the voltaite group: solid solutions, Mössbauer and infrared spectra, and anomalous anisotropy	J. Majzlan, H. Schlicht, M. Wierzbicka-Wieczorek, G. Giester, H. Pöllmann, B. Brömme, S. Doyle, G. Buth, C. Bender Koch	Miner. Petrol. 107, 221-233	2013	PDF
High resolution synchrotron X-ray studies of phase separation phenomena and the scaling law for the threading dislocation densities reduction in high quality AIGaN heterostructure	S. Lazarev, S. Bauer, K. Forghani, M. Barchuk, F. Scholz, T. Baumbach	Journal of Crystal Growth 370, 51-56	2013	PDF
Three-dimensional reciprocal space mapping of diffuse scattering for the study of stacking faults in semipolar (1122) GaN layers grown from the sidewall of an r-patterned sapphire substrate	S. Lazarev, S. Bauer, T. Meisch, M. Bauer, I. Tischer, M. Barchuk, K. Thonke, V. Holy, F. Scholz, T. Baumbach	J. Appl. Cryst. 46, 1425-1433	2013	PDF
Study of threading dislocation density reduction in AlGaN epilayers by Monte Carlo simulation of high-resolution reciprocal-space maps of a two-layer system	S. Lazarev, M. Barchuk, S. Bauer, K. Forghani, V. Holý, F. Scholz, T. Baumbach	J. Appl. Cryst. 46, 120-127	2013	PDF
Determination of nanoscale heat conductivity by time-resolved X-ray scattering	D. Issenmann, N. Wehmeier, S. Eon, H. Bracht, G. Buth, S. Ibrahimkutty, A. Plech	Thin Solid Films 541, 28-31	2013	PDF
Mechanical and Morphological Properties of a Ternary Polyamide 6 Nanocomposite With Optimized Stiffness/Toughness Performance	S. Geier, C. Bonten	Polymer Eng. Sci. 54, 247-254	2013	PDF
Experimental Test of Data Analysis Methods from Staggered Pair X-ray Beam Position Monitors at Bending Magnet Beamlines	G. Buth, E. Huttel, S. Mangold, R. Steininger, D. Batchelor, S. Doyle, R. Simon	J. Phys.: Conf. Ser. 425, 042004	2013	PDF
Ringing the changes in FeIII/YbIII cyclic coordination clusters	A. Baniodeh, C. E. Anson, A. K. Powell	Chem. Sci. 4, 4354-4361	2013	PDF
Magnetic Interactions Mediated by Diamagnetic Cations in [Mn18M](M = Sr2+,Y3+,Cd2+, and Lu3+) Coordination Clusters	A. M. Ako, B. Burger, Y. Lan, V. Mereacre, R. Clerac, G. Buth, S. Gomez-Coca, E. Ruiz, C. E. Anson, A. K. Powell	Inorg. Chem. 52, 5764-5774	2013	PDF
Synthesis, Magnetism, and 57Fe Mössbauer Spectroscopic Study of a Family of [Ln3Fe7] Coordination Clusters (Ln = Gd, Tb, and Er)	G. Abbas, Y. Lan, V. Mereacre, G. Buth, M. T. Sougrati, F. Grandjean, G. J. Long, C. E. Anson, A. K. Powell	Inorg. Chem. 52, 11767-11777	2013	PDF
Modular Palladium Bipyrazoles for the Isomerization of Allylbenzenes - Mechanistic Considerations and Insights into Catalyst Design and Activity, Role of Solvent, and Additive Effects	M. J. Spallek, S. Stockinger, R. Goddard, O. Trapp	Advanced Synthesis & Catalysis 354 (2012) 1466-1480	2012	PDF
Probing the Influence of Size and Composition on the Photoelectron Spectra of Cadmium Chalcogenide Cluster Dianions	K. Matheis, A. Eichhoefer, F. Weigend, O. T. Ehrler, O. Hampe, M. M. Kappes	Journal of Physical Chemistry C 116 (2012) 13800-13809	2012	PDF
X-ray study of surface layers of air-annealed Be12Ti and Be12V samples using synchrotron radiation	P. Kurinskiy, A. Moeslang, V. Chakin, T. Slobodskyy, A. A. Minkevich, T. Baumbach, Ch. Dorn, A. A. Goraieb	Fusion Engineering and Design 87 (2012) 872-875	2012	PDF
Water coordinated zinc dioxo-chlorin and porphyrin self-assemblies as chlorosomal mimics: variability of supramolecular interactions	A. Jesorka, A. R. Holzwarth, A. Eichhöfer, C. M. Reddy, Y. Kinoshita, H. Tamiaki, M. Katterle, J.-V. Naubron, T. S. Balaban	Photochemical & Photobiological Sciences 11 (2012) 1069-1080	2012	PDF
Lattice Dynamics of Laser Excited Ferroelectric BaTiO3	D. Issenmann, S. Schleef, S. Ibrahimkutty, G. Buth, T. Baumbach, A. Plech, M. Beyer, J. Demsar	Acta Physica Polonica A 121 (2012) 319-323	2012	PDF
Constructing Single-Chain Magnets by Supramolecular p–p Stacking and Spin Canting: A Case Study on Manganese(III) Corroles	M. Ding, B. Wang, Z. Wang, J. Zhang, O. Fuhr, D. Fenske, S. Gao	Chemistry - A European Journal 18 (2012) 915-924	2012	PDF
Self-Assembly of a Mononuclear (FEIII(L)(EtOH2) Complex Bearing an n-Dodedyl Chain on Solid Highly oriented Pyrolytic Graphite Surfaces	A. M. Ako, Sahabul Alam M., M. Rahman, J. P. Hill, N. M. Sanchez-Ballester, K. Ariga, G. Buth, C. E. Anson, A. K. Powell	Chemistry - A European Journal 18 (2012) 16419-16425	2012	PDF
The Rhenium Tris(dithiolene) Electron Transfer Series: Calibrating Covalency	S. Sproules, T. Weyhermüller, R. Goddard, K. Wieghardt	Inorganic Chemistry 50 (2011) 12623-12631	2011
The Formal Combination of Three Singlet Biradicaloid Entities to a Singlet Hexaradicaloid Metalloid Ge14[Si(SiMe3)3]5[Li(THF)2]3 Cluster	C. Schenk, A. Kracke, K. Fink, A. Kubas, W. Klopper, M. Neumaier, H. Schnöckel, A. Schnepf	Journal of the American Chemical Society 133 (2011) 2518-2524	2011
Contribution of Spin and Anisotropy to Single Molecule Magnet Behavior in a Family of Bell-Shaped Mn11Ln2 Coordination Clusters	V. Mereacre, Y. Lan, R. Clérac, A. M. Ako, W. Wernsdorfer, G. Buth, C. E. Anson, A. K. Powell	Inorganic Chemistry 50 (2011) 12001-12009	2011
Intermolecular interactions, disorder and twinning in ciprofloxacin–2,2-difluoroethanol (2/3) and ciprofloxacin–water (3/14.5)	F. P. A. Fabbiani, J.-B. Arlin, G. Buth, B. Dittrich, A. J. Florence, R. Herbst-Irmer, H. Sowa	Acta Crystallographica Section C - Crystal Structure Communications 67 (2011) o120-o124	2011
Homoleptic 1-D iron selenolate complexes-synthesis, structure, magnetic and thermal behaviour of (1)(infinity)[Fe(SeR)(2)] (R = Ph, Mes)	A. Eichhöfer, G. Buth, F. Dolci, K. Fink, R. A. Mole, P. T. Wood	Dalton Transactions 40 (2011) 7022-7032	2011
Investigation of crystallographic and detection properties of CdTe at the ANKA synchrotron light source	A. Cecilia, E. Hamann, C. Haas, D. Greiffenberg, A. N. Danilewsky, D. Haenscke, A. Fauler, A. Zwerger, G. Buth, P. Vagovic, T. Baumbach, M. Fiederle	Journal of Instrumentation 6 (2011) DOI: 10.1088/1748-0221/6/10/P10016	2011
Grazing-incidence x-ray diffraction from GaN epitaxial layers with threading dislocations	M. Barchuk, V. Holy, B. Miljevic, B. Krause, T. Baumbach	Applied Physics Letters 98 (2011) 021912-1-3	2011
Lateral ordering, strain, and morphology evolution of InGaAs/GaAs(001) quantum dots due to high temperature postgrowth annealing	M. Riotte, E. Fohtung, D. Grigoriev, A. A. Minkevich, T. Slobodskyy, M. Schmidbauer, T. H. Metzger, D. Z. Hu, D. M. Schaadt, T. Baumbach	Applied Physics Letters 96 (2010) 083102-1-3	2010
Comparative study of multilayers used in monochromators for synchrotron-based coherent hard X-ray imaging	A. Rack, T. Weitkamp, M. Riotte, D. Grigoriev, T. Rack, L. Helfen, T. Baumbach, R. Dietsch, T. Holz, M. Krämer, F. Siewert, M. Meduna, P. Cloetens, E. Ziegler	Journal of Synchrotron Radiation 17 (2010) 496-510	2010
Family of MnIII2Ln2(µ4-O) Compounds: Syntheses, Structures, and Magnetic Properties	V. Mereacre, Y. Lan, R. Clerac, A. M. Ako, I. J. Hewitt, W. Wernsdorfer, G. Buth, C. E. Anson, A. K. Powell	Inorganic Chemistry 49 (2010) 5293-5302	2010
New heterometallic [MnIII4LnIII4] wheels incorporating formate ligands	M. Li, A. M. Ako, Y. Lan, W. Wernsdorfer, G. Buth, C. E. Anson, A. K. Powell, Z. Wang, S. Gao	Dalton Transactions 39 (2010) 3375-3377	2010
A Family of 3d-4f Octa-Nuclear [MnIII4LnIII4] Wheels (Ln = Sm, Gd, Tb, Dy, Ho, Er, and Y): Synthesis, Structure, and Magnetism	M. Li, Y. Lan, A. M. Ako, W. Wernsdorfer, C. E. Anson, G. Buth, A. K. Powell, Z. Wang, S. Gao	Inorganic Chemistry 49 (2010) 11587-11594	2010
Searching for novel crystal forms by in situ high-pressure crystallisation: the example of gabapentin heptahydrate	F. P. A. Fabbiani, D. C. Levendis, G. Buth, W. F. Kuhs, N. Shankland, H. Sowa	CrystEngComm 12 (2010) 2354-2360	2010
Pressure-induced structural changes in wet vitamin B12	F. P. A. Fabbiani, G. Buth, B. Dittrich, H. Sowa	CrystEngComm 12 (2010) 2541-2550	2010
1-D-Tin(II) Phenylchalcogenolato Complexes 81[Sn(EPh)2] (E = S, Se, Te) – Synthesis, Structures, Quantum Chemical Studies and Thermal Behaviour	A. Eichhöfer, J.-J. Jiang, H. Sommer, F. Weigend, O. Fuhr, D. Fenske, C.-Y. Su, G. Buth	European Journal of Inorganic Chemistry 2010 (2010) 410-418	2010